CN104017577B - A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia - Google Patents
A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia Download PDFInfo
- Publication number
- CN104017577B CN104017577B CN201410280832.3A CN201410280832A CN104017577B CN 104017577 B CN104017577 B CN 104017577B CN 201410280832 A CN201410280832 A CN 201410280832A CN 104017577 B CN104017577 B CN 104017577B
- Authority
- CN
- China
- Prior art keywords
- quantum dot
- pentanedione
- acetylacetone
- carbon quantum
- ammonia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia.Concretely comprise the following steps, pipette a certain amount of acetylacetone,2,4-pentanedione and ammonia adds in suitable quantity of water, stir in round-bottomed flask, heating a period of time, by reacted solution, first rotary evaporation at least quantity of fluid, transfer in chromatographic column, carry out eluting, thus obtaining nitrogen-doped carbon quantum dot.This preparation method mild condition, reaction green, agents useful for same are simple, are a kind of methods having application prospect.
Description
Technical field
The invention belongs to carbon quantum dot preparing technical field, relate to a kind of nitrogen-doped carbon quantum dot synthetic method being carbon source with acetylacetone,2,4-pentanedione.
Background technology
Fluorescent carbon quantum dot is owing to having a wide range of applications in fields such as biomarker, bio-imaging, pharmaceutical carrier, photoelectric devices, and has better biocompatibility and hypotoxicity than conventional semiconductors quantum dot so that it is paid close attention to widely.
Through retrieval, publication number is the Chinese invention patent of CN102897745A, discloses " a kind of method utilizing conjugated polymer to prepare carbon quantum dot and application thereof ".It is characterized in that comprising the following steps: by adding the aqueous solution of 0.01～1000 times of conjugated polymer quality, the acid of 0～1M or alkali, mix homogeneously in conjugated polymer, obtain reactant liquor；The reactant liquor of mix homogeneously is proceeded to reactor, reacts 1～24 hour under 100 DEG C～500 DEG C conditions；It is cooled to room temperature after having reacted, collects reactant liquor, separating-purifying, obtain carbon quantum dot；Carbon quantum dot prepared by the present invention is with low cost, it is possible to achieve preparation in macroscopic quantity, and productivity is high, good water solubility and nontoxic, is the aspects such as biomarker, fluorescence sense and the photo-thermal therapy cancer inorganic nonmetallic nanometer material with major application prospect.
Publication number is the Chinese invention patent of CN102745669A, discloses " preparation method of luminescence generated by light carbon quantum dot ".It is characterized in that comprising the following steps: Semen sojae atricolor solid residue after squeezing bean milk is dried dehydration, insert heating carbonization in electric drying oven with forced convection, it is thus achieved that the crude product of carbon quantum dot；Carbon quantum dot crude product is ground, sieves, and disperse in deionized water, to stir, stand, centrifugal, the aqueous solution obtained containing carbon quantum dot is evaporated, lyophilization is to Powdered, thus finally obtaining luminescence generated by light carbon quantum dot.The method adopting the present invention prepares luminescence generated by light carbon quantum dot, and using household soy milk machine to obtain bean dregs is raw material, and raw material sources are extensive, prepared by low-temperature heat carbonization, simple to operate, cost is low, and yield is high, preparation technology device simple, and operation can be completed in very short time, it is easy to promote.
Those skilled in the art is devoted to develop a kind of mild condition, reaction green, the simple nitrogen-doped carbon quantum dot preparation method of agents useful for same.
Summary of the invention
Because the defect of prior art, the technical problem to be solved is to adopt acetylacetone,2,4-pentanedione and ammonia to be reaction raw materials and provide a kind of method directly heating synthetic nitrogen doping carbon quantum dot.
For achieving the above object, the invention provides a kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia: pipette a certain amount of acetylacetone,2,4-pentanedione and ammonia adds in suitable quantity of water, round-bottomed flask stirs, heating a period of time, by reacted solution, first rotary evaporation at least quantity of fluid, transfer on silicagel column, carry out eluting, thus obtaining nitrogen-doped carbon quantum dot.Specifically comprising the following steps that of the method
A. pipette a certain amount of acetylacetone,2,4-pentanedione and ammonia adds in suitable quantity of water, stir in round-bottomed flask, heat a period of time；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer in chromatographic column, carry out eluting, thus obtaining nitrogen-doped carbon quantum dot.
Preferably, the volume of acetylacetone,2,4-pentanedione is 1～10ml.
Preferably, the volume of ammonia is 1～10ml.
Preferably, the volume of water is 10～100ml.
Preferably, in step a, heating-up temperature is 60～90 DEG C.
Preferably, in step a, heat time heating time is 5～24h.
Preferably, in step b, chromatographic column is silicagel column, and the height of silicagel column is the 1/3～2/3 of chromatographic column height.
Preferably, the eluent that step b selects is dichloromethane or the mixed liquor of dichloromethane and methanol.
It is highly preferred that eluent by dichloromethane and methanol according to volume ratio dichloromethane: methanol=1:0～1:1 is mixed to form.
Compared with prior art, the solution have the advantages that: reaction condition is gentle, reaction green, and agents useful for same is simple, is a kind of method having application prospect.
Accompanying drawing explanation
Fig. 1 is overall flow schematic diagram of the present invention；
Fig. 2 is the photoluminescence laser spectrum figure of the embodiment of the present invention 1 synthetic nitrogen doping carbon quantum dot；
Fig. 3 is the transmission electron microscopy figure of the embodiment of the present invention 1 synthetic nitrogen doping carbon quantum dot.
Detailed description of the invention
Embodiment 1
A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia, specifically comprises the following steps that
A. pipette 1ml acetylacetone,2,4-pentanedione and 1ml ammonia adds in 25ml water, stir in round-bottomed flask, heat 9h in 60 DEG C；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer on silicagel column, the height of silicagel column is at 1/3 place of chromatographic column, and eluent is dichloromethane, carries out eluting, thus obtaining nitrogen-doped carbon quantum dot.
Embodiment 2
A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia, specifically comprises the following steps that
A. pipette 1ml acetylacetone,2,4-pentanedione and 1ml ammonia adds in 25ml water, stir in round-bottomed flask, heat 24h in 70 DEG C；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer on silicagel column, the height of silicagel column is at 1/2 place of chromatographic column, and eluent is dichloromethane and the methyl alcohol mixed liquor of volume ratio 2:1, carries out eluting, thus obtaining nitrogen-doped carbon quantum dot.
Embodiment 3
A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia, specifically comprises the following steps that
A. pipette in the water of 2ml acetylacetone,2,4-pentanedione and 2ml ammonia addition 50ml, stir in round-bottomed flask, heat 5h in 90 DEG C；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer on silicagel column, the height of silicagel column is at 2/3 place of chromatographic column, and eluent is dichloromethane and the methyl alcohol mixed liquor of volume ratio 1:1, carries out eluting, thus obtaining nitrogen-doped carbon quantum dot.
Embodiment 4
A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia, specifically comprises the following steps that
A. pipette in the water of 1ml acetylacetone,2,4-pentanedione and 1ml ammonia addition 10ml, stir in round-bottomed flask, heat 5h in 60 DEG C；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer on silicagel column, the height of silicagel column is at 1/3 place of chromatographic column, and eluent is dichloromethane and the methyl alcohol mixed liquor of volume ratio 1:1, carries out eluting, thus obtaining nitrogen-doped carbon quantum dot.
Embodiment 5
A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia, specifically comprises the following steps that
A. pipette in the water of 10ml acetylacetone,2,4-pentanedione and 10ml ammonia addition 100ml, stir in round-bottomed flask, heat 24h in 80 DEG C；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer on silicagel column, the height of silicagel column is at 2/3 place of chromatographic column, and eluent is dichloromethane and the methyl alcohol mixed liquor of volume ratio 1:1, carries out eluting, thus obtaining nitrogen-doped carbon quantum dot.
The preferred embodiment of the present invention described in detail above.Should be appreciated that those of ordinary skill in the art just can make many modifications and variations according to the design of the present invention without creative work.Therefore, all technical staff in the art, all should in the protection domain being defined in the patent claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (7)
1. the method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia, it is characterised in that the method comprises the following steps:
A. pipette acetylacetone,2,4-pentanedione and ammonia adds in suitable quantity of water, stirring 60～90 DEG C of heating 5～24h in round-bottomed flask；
B. by reacted solution, first rotary evaporation at least quantity of fluid, transfer in chromatographic column, carry out eluting, thus obtaining nitrogen-doped carbon quantum dot.
2. the method being directly synthesized nitrogen-doped carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia heating according to claim 1, it is characterised in that the volume of described acetylacetone,2,4-pentanedione is 1～10ml.
3. the method being directly synthesized nitrogen-doped carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia heating according to claim 1, it is characterised in that the volume of described ammonia is 1～10ml.
4. the method being directly synthesized nitrogen-doped carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia heating according to claim 1, it is characterised in that the volume of described water is 10～100ml.
5. the method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia according to claim 1, it is characterised in that chromatographic column described in step b is silicagel column, the height of described silicagel column is the 1/3～2/3 of chromatographic column height.
6. the method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia according to claim 1, it is characterised in that the eluent that step b selects is dichloromethane or the mixed liquor of dichloromethane and methanol.
7. the method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia according to claim 6, it is characterised in that described eluent by dichloromethane and methanol according to volume ratio dichloromethane: methanol=1:0～1:1 is mixed to form.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410280832.3A CN104017577B (en) | 2014-06-20 | 2014-06-20 | A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410280832.3A CN104017577B (en) | 2014-06-20 | 2014-06-20 | A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104017577A CN104017577A (en) | 2014-09-03 |
| CN104017577B true CN104017577B (en) | 2016-07-06 |
Family
ID=51434589
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410280832.3A Active CN104017577B (en) | 2014-06-20 | 2014-06-20 | A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104017577B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104403665A (en) * | 2014-12-10 | 2015-03-11 | 东华大学 | Method for preparing nitrogen doped carbon quantum dots by using shrimp waste |
| CN104569375A (en) * | 2015-01-29 | 2015-04-29 | 三诺生物传感股份有限公司 | Method for preparing fluorescent carbon quantum dot |
| CN104927848B (en) * | 2015-06-16 | 2017-03-29 | 复旦大学 | Material of bio-imaging probe and oxygen reduction catalyst and preparation method thereof |
| CN105236383B (en) * | 2015-09-14 | 2017-07-07 | 复旦大学 | Carbon quantum dot of Wavelength tunable and its preparation method and application |
| CN105670617A (en) * | 2016-01-14 | 2016-06-15 | 中国石油大学(华东) | Simple efficient one-step method for batch preparation of nitrogen-doped petroleum coke-based carbon quantum dots |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436257A (en) * | 2013-08-27 | 2013-12-11 | 湖南师范大学 | Method for preparing fluorescent carbon dots (C-dots) through electrochemical carbonization of ketone |
| CN103663412A (en) * | 2013-12-05 | 2014-03-26 | 中国科学院大学 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8357507B2 (en) * | 2010-03-08 | 2013-01-22 | Cromoz Inc. | Water soluble fluorescent quantum carbon dots |
| CN103497762B (en) * | 2013-06-26 | 2015-03-25 | 上海交通大学 | Method for synthesizing nitrogen doped carbon quantum dot based on one-step monocomponent hydro-thermal synthesis |
-
2014
- 2014-06-20 CN CN201410280832.3A patent/CN104017577B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436257A (en) * | 2013-08-27 | 2013-12-11 | 湖南师范大学 | Method for preparing fluorescent carbon dots (C-dots) through electrochemical carbonization of ketone |
| CN103663412A (en) * | 2013-12-05 | 2014-03-26 | 中国科学院大学 | Preparation method of carbon quantum dots with adjustable fluorescence colors |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104017577A (en) | 2014-09-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104017577B (en) | A kind of method directly heating synthetic nitrogen doping carbon quantum dot based on acetylacetone,2,4-pentanedione and ammonia | |
| CN104017576B (en) | A kind of method based on citrate of lime and urea microwave reaction synthetic nitrogen doping carbon quantum dot | |
| CN104192827A (en) | Method for synthesizing carbon quantum dots on basis of organic micromolecule microwave solid-phase reaction | |
| CN106190126B (en) | Monodisperse near-infrared silver telluride quantum dot and preparation method thereof | |
| CN103484111B (en) | Mesoporous silicon fluorescent material and preparation method | |
| CN105647526A (en) | Near-full-spectrum fluorescent nanocarbon dots and preparation method thereof | |
| CN107774294A (en) | A kind of novel photochemical catalyst K g C3N4And its prepare and apply | |
| CN104845619A (en) | Rapid synthesis method for high-quantum-yield fluorescent carbon dots | |
| CN107418572A (en) | A kind of method that sonochemical method prepares caesium lead bromine perovskite quantum dot | |
| CN108192604A (en) | A kind of preparation method of nitrogen-doped graphene quantum dot | |
| CN104987861A (en) | Method for preparing carbon dots with up-down conversion luminescence characteristic from maize straw | |
| CN108467730A (en) | A method of preparing fluorescent carbon point | |
| CN104263366A (en) | Red-light emission fluorescent carbon dot with up and down conversion function and preparation method of red-light emission fluorescent carbon dot | |
| CN105032486A (en) | Preparation method of spindle-shaped metal organic framework compound grains | |
| CN107651708A (en) | A kind of method that microwave hydrothermal prepares 1T@2H MoS2 | |
| CN104560035A (en) | Carbon quantum dot fluorescence labeling material with orange peels used as carbon source as well as preparation method and application of carbon quantum dot fluorescence labeling material | |
| CN109701535A (en) | Cuprous oxide-carbon dots-copper Three-element composite photocatalyst preparation method | |
| CN104479674B (en) | Take Xylene Brilliant Cyanine G as the method that carbon source prepares near infrared carbon quantum dot | |
| CN106978170B (en) | A kind of preparation method of water-solubility fluorescent carbon quantum dot | |
| CN102504821A (en) | Preparation method of rare earth-doped sodium gadolinium tetrafluoride nanomaterial | |
| CN104560036A (en) | Carbon quantum dot fluorescence-labeled material adopting honey as carbon source, as well as preparation method and application thereof | |
| CN105668605B (en) | A kind of nest like has the preparation method of high specific surface area and mesoporous ceria | |
| CN104962283B (en) | Preparation method of chlorine/phosphorus-codoped carbon quantum dots | |
| CN205007627U (en) | Multi -functional traditional chinese medicine extraction element | |
| CN107572501B (en) | Preparation method of high-yield carbon quantum dots |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |